CN116102056A - Superfine titanium dioxide powder and preparation method thereof - Google Patents
Superfine titanium dioxide powder and preparation method thereof Download PDFInfo
- Publication number
- CN116102056A CN116102056A CN202211433576.8A CN202211433576A CN116102056A CN 116102056 A CN116102056 A CN 116102056A CN 202211433576 A CN202211433576 A CN 202211433576A CN 116102056 A CN116102056 A CN 116102056A
- Authority
- CN
- China
- Prior art keywords
- titanium dioxide
- dioxide powder
- superfine
- solution
- preparing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 162
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 77
- 239000000843 powder Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 26
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 25
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 19
- 230000007062 hydrolysis Effects 0.000 claims abstract description 16
- 239000010936 titanium Substances 0.000 claims abstract description 14
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000012452 mother liquor Substances 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- -1 titanium oxide compound Chemical class 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 17
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 15
- 229910052744 lithium Inorganic materials 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000010413 mother solution Substances 0.000 claims description 7
- 239000007773 negative electrode material Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000003828 vacuum filtration Methods 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 10
- 229910001416 lithium ion Inorganic materials 0.000 description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000003917 TEM image Methods 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000002336 sorption--desorption measurement Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 150000003609 titanium compounds Chemical class 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000010405 anode material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000013139 quantization Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses superfine titanium dioxide powder and a preparation method thereof, belonging to the field of inorganic chemical industry. The preparation method of the superfine titanium dioxide powder comprises the following steps: a. preparing titanium powder into titanium-containing solution, adding ammonia water and hydrogen peroxide for full reaction; b. c, fully reacting the solution obtained in the step a with hydrolysis mother liquor, performing solid-liquid separation and drying treatment to obtain a titanium oxide compound precursor; c. and (3) carrying out heat treatment on the titanium oxide precursor for 2-4 hours in an air atmosphere at 300-450 ℃ to obtain the superfine titanium dioxide powder. The specific surface area of the superfine titanium dioxide powder prepared by the invention is up to 260m 2 Per gram, the electrochemical capacity can reach 180mAh g under 0.1C multiplying power ‑1 The method has simple working procedures and lower cost, and can effectively solve the problem of higher cost of the existing method for preparing the superfine titanium dioxide。
Description
Technical Field
The invention belongs to the field of inorganic chemical industry, and in particular relates to superfine titanium dioxide powder and a preparation method thereof.
Background
The technical core of the lithium ion battery is electrode system pairing, and the lithium ion battery is expanded to the reasonable selection of other parts on the basis of the electrode system pairing. The initial pairing mode of lithium batteries is based on metallic lithium negative electrode and TiS 2 The pairing mode of the positive electrode can prepare a lithium ion secondary battery with high energy density based on the pairing mode, the lithium ion secondary battery using metallic lithium as the negative electrode can obtain higher energy density and power density, but the secondary battery using metallic lithium as the negative electrode can generate metallic lithium crystal branches on the surface of the negative electrode due to uneven atomic scale of the surface of a metallic lithium sheet in the charging and discharging process, thereby not only causing Li + And can cause the boule to pierce the diaphragm to produce a safety accident. Therefore, a new lithium battery electrode pairing mode needs to be found.
Titanium-based material (TiO 2 ) As an emerging anode material capable of replacing carbon-based materials, the anode material has a charge-discharge voltage plateau height of 1.65VVS Li/Li + High safety, good charge-discharge cycle performance and the like. Can be used as the negative electrode material of lithium ion power batteries, and can also be used as the negative electrode material of lithium ion secondary batteries such as automobile power batteries and large-scale energy storage. The titanium dioxide material has the advantages of stable structure, safety, no toxicity, wide sources and the like, and is widely used as a filler, a brightening agent, a catalyst, a battery electrode material and the like. The particle size of the titanium dioxide material is an important material quantization index in the use process, and the titanium dioxide material has higher specific surface area and higher heterogeneous contact area under the same mass, so that series of advantages are brought. The superfine titanium dioxide powder is directly used as a lithium ion battery cathode material, and due to the ultrahigh specific surface area, the wettability of the electrode material in the electrolyte can be improved, the diffusion distance of Li+ in the electrode material can be shortened, and the overall electrochemical performance of the lithium ion battery cathode titanium dioxide can be improved.
Patent CN113896233a discloses a method for preparing low-temperature crystallized titanium dioxide; patent CN114162860a discloses a preparation method of titanium dioxide porous spheres; patent CN113912109a discloses a preparation method of a nano titanium dioxide porous material; patent CN113957506a discloses a preparation method of rutile type titanium dioxide board; patent CN113896234a discloses a method for preparing nano titanium dioxide; patent CN114906873a discloses a process for preparing anatase titanium dioxide. In the prior art, there are various preparation methods of titanium dioxide, wherein most of the preparation methods are based on the technological process of titanium dioxide by a sulfuric acid method (as shown in fig. 1), namely, intermediate products in the production process of titanium dioxide by the sulfuric acid method are used as raw materials, and hydrothermal reaction is used for preparing corresponding nano titanium dioxide, such as patent CN113896234A, CN113896233A, CN114162860A; or other substances are used to make nano titanium dioxide with a core-shell structure, such as patent CN113912109A; or based on basic sulfuric acid process titanium dioxide production technology, titanium dioxide can be prepared, such as patent CN114906873A.
The prior art for preparing ultrafine titanium dioxide mostly needs complicated process flow and expensive equipment, or needs other auxiliary materials with high cost, and has high production cost, so that research on a new preparation method of ultrafine titanium dioxide is needed.
Disclosure of Invention
The invention aims to solve the technical problem that the existing method for preparing superfine titanium dioxide has higher cost.
The technical scheme adopted for solving the technical problems is as follows: the preparation method of the superfine titanium dioxide powder comprises the following steps:
a. preparing titanium powder into a titanium-containing solution, adding ammonia water to adjust the pH of the solution to 10-12, and then adding hydrogen peroxide to fully react to obtain a dissolved precursor solution;
b. c, adding the dissolved precursor solution obtained in the step a into hydrolysis mother liquor for full reaction, and then carrying out solid-liquid separation to obtain white particle precipitation and drying treatment to obtain a titanium oxide compound precursor;
c. and c, putting the titanium oxide precursor obtained in the step b into a vacuum tube furnace, and heating from normal temperature to 300-450 ℃ for 2-4 hours at a heating rate of 5 ℃/min under the air atmosphere to obtain the superfine titanium dioxide powder.
In the step a, the mass ratio of the titanium powder to the water in the titanium-containing solution is 0.5-2%, and the addition amount of the hydrogen peroxide is 20-40% of the volume of the water.
Further, the hydrogen peroxide is a hydrogen peroxide solution having a concentration of 30%.
In the step a, the reaction is carried out for 1-3h under the condition of stirring.
In the step b, the volume ratio of the dissolved precursor solution to the hydrolysis mother solution is 1-5:100.
In the step b, the hydrolysis mother solution is an ammonia water solution with the pH value of 8-12.
In the step b, the dissolved precursor solution is slowly added under stirring at normal temperature.
Further, the normal temperature is 25-28 ℃.
In the step b, the hydrolysis reaction is carried out for 12-36h under the condition of stirring.
In the step b, the solid-liquid separation mode adopts vacuum filtration separation.
In the step b, the drying treatment is vacuum drying at 80-100 ℃ for 12-24h.
The superfine titanium dioxide powder capable of being directly used as the negative electrode material of the lithium battery is prepared by the preparation method of the superfine titanium dioxide powder.
The beneficial effects of the invention are as follows: according to the invention, metallic titanium powder is used as a basic titanium source, and is utilized to react with hydrogen peroxide and ammonia water in a dissolving way to generate a hydrolysis precursor, and a great amount of heat generated in the metal dissolving process can generate a hydrolysis precursor with finer particles in the subsequent hydrolysis process according to the law of conservation of energy, and then the lower heat treatment temperature is continued, so that the superfine titanium dioxide powder is finally obtained.
The specific surface area of the superfine titanium dioxide powder prepared by the invention is up to 260m 2 Per gram, the electrochemical capacity can reach 180mAh g under 0.1C multiplying power -1 The product of the invention has higher electrochemical performance, can be directly used as a lithium battery negative electrode material, can be used as a titanium source to prepare a lithium titanate material, and can be used as a lithium battery negative electrode material. Comprehensive synthesisAnalyzing the current development situation in the field of lithium batteries, the titanium-based material as a negative electrode of the lithium battery has wider development prospect in the future; the preparation method disclosed by the invention is simple in procedure, does not need to apply complex equipment and instruments, does not need to use expensive auxiliary materials, and is low in production cost, so that the technical scheme disclosed by the invention has high popularization value.
Drawings
FIG. 1 is a schematic flow chart of a conventional sulfuric acid process titanium dioxide production process in the prior art;
FIG. 2 is a TEM image of a conventional titanium dioxide powder;
FIG. 3 is a TEM image of the ultrafine titanium dioxide powder prepared in example 1 of the invention;
FIG. 4 is a diagram of N of a conventional titanium dioxide powder 2 Adsorption/desorption isotherms;
FIG. 5 is a drawing showing N of ultrafine titanium dioxide powder prepared in example 1 of the present invention 2 Adsorption/desorption isotherms;
FIG. 6 is a graph showing the charge-discharge capacity versus voltage of the ultrafine titanium dioxide powder prepared in example 1 of the present invention.
Detailed Description
The technical scheme of the invention can be implemented in the following way.
The preparation method of the superfine titanium dioxide powder comprises the following steps:
a. dissolving metallic titanium powder into the solution under normal temperature to form a titanium-containing solution, wherein the mass ratio of the adding amount of the titanium powder to water is 0.5-2%; adding ammonia water under stirring at normal temperature to control the pH value of the solution to be between 10 and 12, then adding hydrogen peroxide (hydrogen peroxide solution with the concentration of 30 percent) with the addition amount of 20 to 40 percent of the volume of water, and stirring and reacting for 1 to 3 hours until yellow flocculent precipitate is generated to obtain a dissolved precursor solution;
b. c, adjusting the pH value of the aqueous solution to 8-12 (ammonia water solution), wherein the temperature is 25-28 ℃ at normal temperature, slowly adding the dissolved precursor solution obtained in the step a into the aqueous solution, wherein the volume ratio of the added amount of yellow floccules to water is 1-5:100, and carrying out hydrolysis reaction for 12-36h under the stirring condition to obtain a solution filled with white solid particles;
c. and c, separating the solution obtained in the step b through vacuum filtration, filtering solid particles on the paper, and vacuum drying at 80-100 ℃ for 12-24 hours to obtain the titanium oxide precursor.
d. And c, carrying out heat treatment on the titanium oxide precursor in the step c in a vacuum tube furnace at 300-450 ℃ under the air atmosphere for 2-4 hours to obtain superfine titanium dioxide powder.
The superfine titanium dioxide powder capable of being directly used as the negative electrode material of the lithium battery is prepared by the preparation method of the superfine titanium dioxide powder.
The technical scheme and effect of the present invention will be further described by practical examples.
Examples
The invention provides two groups of examples for preparing superfine titanium dioxide powder by adopting the technical scheme of the invention, and the specific experimental steps are as follows.
1. Preparation of ultrafine titanium dioxide
Example 1
200ml of deionized water is measured in a beaker with a measuring cylinder, the beaker is placed in a water bath kettle, an electric stirrer is used for stirring, the rotating speed is set to 300 revolutions per minute, 1g of metallic titanium powder is weighed by a precision balance and added into the beaker, then ammonia water with the mass fraction of 25% is used for regulating the pH value of the solution to 10, 40ml of hydrogen peroxide is added after stirring for 10min, and stirring reaction is continued for 1h, so that a dissolved precursor solution is obtained.
500ml of deionized water is measured in a 1L beaker by using a measuring cylinder, the pH value of the aqueous solution is regulated to 10 by using ammonia water with the mass fraction of 25%, the dissolved precursor solution is slowly added into the hydrolysis mother solution with the pH value of 10, and the hydrolysis mother solution containing the titanium compound is obtained after stirring and reacting for 12 hours at normal temperature.
And (3) filtering the hydrolysis mother liquor containing the titanium compound in vacuum, and then drying the solid matters on the filter paper in vacuum at 90 ℃ for 12 hours to obtain the titanium-containing precursor. And (3) carrying out heat treatment on the titanium-containing precursor in a vacuum tube furnace at the temperature of 300 ℃ in the air atmosphere for 2 hours to obtain superfine titanium dioxide powder.
Example 2
200ml of deionized water is measured in a beaker with a dosage cylinder, the beaker is placed in a water bath kettle, an electric stirrer is used for stirring, the rotating speed is set to 300 revolutions per minute, 2g of metallic titanium powder is taken by precise day translation and added into the beaker, then ammonia water with the mass fraction of 25% is used for regulating the pH value of the solution to be 12, 60ml of hydrogen peroxide is added after stirring for 10min, and stirring reaction is continued for 1h, so that a dissolved precursor solution is obtained.
500ml of deionized water is measured in a 1L beaker by using a measuring cylinder, the pH value of the aqueous solution is regulated to 10 by using ammonia water with the mass fraction of 25%, the dissolved precursor solution is slowly added into the hydrolysis mother solution with the pH value of 10, and the hydrolysis mother solution containing the titanium compound is obtained after stirring reaction for 24 hours at normal temperature.
And (3) filtering the hydrolysis mother liquor containing the titanium compound in vacuum, and then drying the solid matters on the filter paper in vacuum at 90 ℃ for 12 hours to obtain the titanium-containing precursor. And (3) carrying out heat treatment on the titanium-containing precursor in a vacuum tube furnace at the temperature of 400 ℃ in the air atmosphere for 3 hours to obtain the superfine titanium dioxide powder.
2. Performance detection
The invention selects the conventional titanium dioxide powder product as a comparative example, and performs physical and chemical property detection together with the superfine titanium dioxide powder prepared in the embodiment 1 of the invention, and the result is as follows:
(1) TEM test
The conventional titanium dioxide powder and the superfine titanium dioxide powder are respectively subjected to projection electron microscope detection, a conventional titanium dioxide powder TEM image is shown in fig. 2, a superfine titanium dioxide powder TEM image is shown in fig. 3, and the conventional titanium dioxide powder TEM image can be known from fig. 2 and 3: the particle size of the superfine titanium dioxide powder prepared by the invention is obviously lower than that of the conventional titanium dioxide powder.
(2) Specific surface area test
The invention adopts a gas adsorption method to respectively measure the specific surface areas of the conventional titanium dioxide powder and the superfine titanium dioxide powder, and N of the conventional titanium dioxide powder 2 The adsorption/desorption isothermal curves are shown in fig. 4, and the N2 adsorption/desorption isothermal curves of the ultrafine titanium dioxide powder are shown in fig. 5, and can be seen from fig. 4 and 5: the specific surface area of the superfine titanium dioxide powder prepared by the invention reaches 260.6m 2 /g, conventional twoThe specific surface area of the titanium oxide powder is only 24.8m 2 /g。
(3) Electrochemical performance test
The charge and discharge test was performed on the conventional titanium dioxide powder and the ultrafine titanium dioxide powder, respectively, and the charge and discharge capacity-voltage curve of the ultrafine titanium dioxide powder is shown in fig. 6, and as can be seen from fig. 6: the capacity of the superfine titanium dioxide powder prepared by the invention can reach 180mAh g under the multiplying power of 0.1C -1 . Under the identical test condition, the conventional titanium dioxide powder has no electrochemical capacity, and experimental results show that the superfine titanium dioxide powder with the specific surface of titanium dioxide improved can obviously improve the electrochemical activity of the material.
Claims (10)
1. The preparation method of the superfine titanium dioxide powder is characterized by comprising the following steps:
a. preparing titanium powder into a titanium-containing solution, adding ammonia water to adjust the pH of the solution to 10-12, and then adding hydrogen peroxide to fully react to obtain a dissolved precursor solution;
b. c, adding the dissolved precursor solution obtained in the step a into hydrolysis mother liquor for full reaction, and then carrying out solid-liquid separation to obtain white particle precipitation and drying treatment to obtain a titanium oxide compound precursor;
c. and c, putting the titanium oxide precursor obtained in the step b into a vacuum tube furnace, and heating from normal temperature to 300-450 ℃ for 2-4 hours at a heating rate of 5 ℃/min under the air atmosphere to obtain the superfine titanium dioxide powder.
2. The method for preparing ultrafine titanium dioxide powder according to claim 1, wherein: in the step a, the mass ratio of the titanium powder to the water in the titanium-containing solution is 0.5-2%, and the addition amount of the hydrogen peroxide is 20-40% of the volume of the water.
3. The method for preparing ultrafine titanium dioxide powder according to claim 1, wherein: in the step a, the reaction is carried out for 1-3h under the stirring condition.
4. The method for preparing ultrafine titanium dioxide powder according to claim 1, wherein: in the step b, the volume ratio of the dissolved precursor solution to the hydrolysis mother solution is 1-5:100.
5. The method for preparing ultrafine titanium dioxide powder according to claim 1, wherein: in the step b, the hydrolysis mother liquor is ammonia water solution with pH value of 8-12.
6. The method for preparing ultrafine titanium dioxide powder according to claim 1, wherein: in the step b, the dissolved precursor solution is slowly added under the condition of stirring at normal temperature.
7. The method for preparing ultrafine titanium dioxide powder according to claim 6, wherein: the normal temperature is 25-28 ℃.
8. The method for preparing ultrafine titanium dioxide powder according to claim 1, wherein: in the step b, the reaction is hydrolysis reaction for 12-36h under stirring.
9. The method for preparing ultrafine titanium dioxide powder according to claim 1, wherein: in the step b, the solid-liquid separation mode adopts vacuum filtration separation, and the drying treatment is vacuum drying for 12-24 hours at 80-100 ℃.
10. An ultrafine titanium dioxide powder capable of being directly used as a lithium battery negative electrode material, which is prepared by the preparation method of the ultrafine titanium dioxide powder in claims 1-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211433576.8A CN116102056A (en) | 2022-11-16 | 2022-11-16 | Superfine titanium dioxide powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211433576.8A CN116102056A (en) | 2022-11-16 | 2022-11-16 | Superfine titanium dioxide powder and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116102056A true CN116102056A (en) | 2023-05-12 |
Family
ID=86264577
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211433576.8A Pending CN116102056A (en) | 2022-11-16 | 2022-11-16 | Superfine titanium dioxide powder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116102056A (en) |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6602918B1 (en) * | 1999-02-26 | 2003-08-05 | Saga Prefecture | Processes of producing a titanium oxide-forming solution and a dispersion with crystalline titanium oxide particles |
| CN1843937A (en) * | 2006-04-20 | 2006-10-11 | 华中师范大学 | Method for preparing size-controllable electronic grade anatase titania nanopowder |
| JP2006306694A (en) * | 2005-03-29 | 2006-11-09 | Sumitomo Chemical Co Ltd | Titanium oxide precursor |
| CN101333004A (en) * | 2008-06-24 | 2008-12-31 | 中国铝业股份有限公司 | Process for preparing titania microspheres of mesoporous structure |
| CN101559979A (en) * | 2009-05-22 | 2009-10-21 | 东华大学 | Method for preparing extrafine anatase titanium dioxide nano rods |
| JP2010088964A (en) * | 2008-10-03 | 2010-04-22 | Saga Prefecture | Method for producing oxidized titanium particle |
| CN101967010A (en) * | 2010-11-04 | 2011-02-09 | 中南大学 | Method for preparing nano-TiO2 serving as cathode material of lithium ion battery |
| CN102070186A (en) * | 2010-11-23 | 2011-05-25 | 南京航空航天大学 | Preparation method of spinel type nano lithium titanate |
| CN104603059A (en) * | 2013-09-05 | 2015-05-06 | 昭和电工株式会社 | Ultrafine particles of titanium dioxide and method for producing same |
| CN108128803A (en) * | 2018-03-09 | 2018-06-08 | 陕西科技大学 | A kind of method that water-soluble titanium dioxide nano-particle is prepared using titanium valve as presoma |
| CN114920288A (en) * | 2022-07-06 | 2022-08-19 | 安阳工学院 | Method for preparing lithium titanate from high-activity amorphous titanium oxide precursor |
| CN115159564A (en) * | 2022-07-06 | 2022-10-11 | 安阳工学院 | Method for preparing lithium titanate by low-temperature hydrothermal method and application thereof |
-
2022
- 2022-11-16 CN CN202211433576.8A patent/CN116102056A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6602918B1 (en) * | 1999-02-26 | 2003-08-05 | Saga Prefecture | Processes of producing a titanium oxide-forming solution and a dispersion with crystalline titanium oxide particles |
| JP2006306694A (en) * | 2005-03-29 | 2006-11-09 | Sumitomo Chemical Co Ltd | Titanium oxide precursor |
| CN1843937A (en) * | 2006-04-20 | 2006-10-11 | 华中师范大学 | Method for preparing size-controllable electronic grade anatase titania nanopowder |
| CN101333004A (en) * | 2008-06-24 | 2008-12-31 | 中国铝业股份有限公司 | Process for preparing titania microspheres of mesoporous structure |
| JP2010088964A (en) * | 2008-10-03 | 2010-04-22 | Saga Prefecture | Method for producing oxidized titanium particle |
| CN101559979A (en) * | 2009-05-22 | 2009-10-21 | 东华大学 | Method for preparing extrafine anatase titanium dioxide nano rods |
| CN101967010A (en) * | 2010-11-04 | 2011-02-09 | 中南大学 | Method for preparing nano-TiO2 serving as cathode material of lithium ion battery |
| CN102070186A (en) * | 2010-11-23 | 2011-05-25 | 南京航空航天大学 | Preparation method of spinel type nano lithium titanate |
| CN104603059A (en) * | 2013-09-05 | 2015-05-06 | 昭和电工株式会社 | Ultrafine particles of titanium dioxide and method for producing same |
| CN108128803A (en) * | 2018-03-09 | 2018-06-08 | 陕西科技大学 | A kind of method that water-soluble titanium dioxide nano-particle is prepared using titanium valve as presoma |
| CN114920288A (en) * | 2022-07-06 | 2022-08-19 | 安阳工学院 | Method for preparing lithium titanate from high-activity amorphous titanium oxide precursor |
| CN115159564A (en) * | 2022-07-06 | 2022-10-11 | 安阳工学院 | Method for preparing lithium titanate by low-temperature hydrothermal method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110048118B (en) | High-nickel cobalt lithium manganate single crystal precursor, preparation method thereof and high-nickel cobalt lithium manganate single crystal positive electrode material | |
| US10916767B2 (en) | Carbon-coated ternary positive electrode material, preparation method therefor, and lithium ion battery | |
| CN108899480A (en) | A kind of long circulation life height ratio capacity nickel cobalt aluminium positive electrode and preparation method thereof | |
| CN112864365A (en) | Nitrogen-sulfur co-doped porous carbon loaded zinc oxide negative electrode material and preparation method thereof | |
| CN113363492A (en) | Composite coating modified high-nickel NCA positive electrode material and preparation method thereof | |
| CN113620345B (en) | Sodium chromite material and preparation method and application thereof | |
| CN113479860B (en) | SbPO (styrene-ethylene-propylene-diene monomer) 4 Preparation method of nitrogen-doped carbon composite material | |
| CN108598458B (en) | Nitrogen-doped lithium titanate composite material, preparation method thereof and lithium ion battery | |
| CN107742710B (en) | Preparation method of chromium-based lithium ion battery composite negative electrode material | |
| CN106887580B (en) | A kind of lithium ion battery negative material and preparation method thereof | |
| CN117374212A (en) | Positive electrode material, preparation method thereof and positive electrode plate | |
| CN109830772B (en) | Regeneration method of lithium iron phosphate waste | |
| CN115974153A (en) | Method for preparing vanadium oxide containing oxygen defects at low temperature | |
| CN114212764B (en) | Phosphate positive electrode material precursor, preparation method and application thereof | |
| CN116102056A (en) | Superfine titanium dioxide powder and preparation method thereof | |
| CN113363444B (en) | Nano lithium titanate-coated modified graphite negative electrode material, and preparation method and application thereof | |
| CN106207251B (en) | Carbon coating method of hydrothermal lithium iron phosphate | |
| CN111710532B (en) | Antimony trioxide-carbon nanotube composite material and preparation and application thereof | |
| CN107069021A (en) | A kind of preparation method for the negative electrode of lithium titanate battery material that niobium is modified | |
| CN114105141A (en) | Preparation method and application of oxygen-rich functional group carbon material | |
| Zhang et al. | Simple Preparation of Co3O4 with a Controlled Shape and Excellent Lithium Storage Performance | |
| CN110342570A (en) | A kind of preparation method of nano-sheet lithium titanate | |
| CN113451574B (en) | Lithium iron phosphate sheet, preparation method thereof and lithium ion battery | |
| CN108281644B (en) | Molybdenum oxide nano electrode material with mixed morphology and preparation method thereof | |
| CN114368783B (en) | Preparation method of magnesium ion battery anode material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |